模拟移动床色谱分离二十碳五烯酸乙酯和二十二碳六烯酸乙酯  

Separation of eicosapentaenoic acid ethyl ester and docosahexaenoic acid ethyl ester by simulated moving bed chromatography

作　　者：董青 李敏[1] 杨亦文[1] 鲍宗必[1] 杨启炜[1] 张治国[1] 任其龙[1] DONG Qing;LI Min;YANG Yiwen;BAO Zongbi;YANG Qiwei;ZHANG Zhiguo;REN Qilong(Key Laboratory of Biomass Chemical Engineering of Ministry of Education,College of Chemical and Biological Engineering,Zhejiang University,Hangzhou 310027,China)

机构地区：[1]浙江大学化学工程与生物工程学院,生物质化工教育部重点实验室,浙江杭州310027

出　　处：《色谱》2018年第9期858-865,共8页Chinese Journal of Chromatography

基　　金：国家自然科学基金面上项目(21776240);国家自然科学基金重点项目(21436010);浙江省重点科技创新团队计划(2011R50002).

摘　　要：二十碳五烯酸和二十二碳六烯酸是两种非常重要的ω-3多不饱和脂肪酸,广泛用于膳食补充剂和药品,同时它们的生理作用并不完全相同,因此分离制备它们的高纯度单体十分必要。首先以聚苯乙烯/二乙烯基苯(PS/DVB)聚合物为固定相,在液相色谱上分离二十碳五烯酸乙酯(EPA-EE)和二十二碳六烯酸乙酯(DHA-EE),考察了流动相、填料粒径、温度对分离的影响。然后采用粒径20μm、孔径10 nm的PS/DVB填料装填了8根150 mm×10 mm的半制备色谱柱,测定了半制备柱装填的均一性。最后尝试在模拟移动床(SMB)色谱上分离EPA-EE和DHA-EE的混合物,探究了Ⅱ区和Ⅲ区的流量、进料流量、进料浓度对分离的影响,结果表明SMB制备的EPA-EE和DHA-EE的相对纯度分别为91.6%和93.6%,回收率分别为97.0%和91.6%,固定相生产率为5.97 g/(L·h),溶剂消耗为1.52 L/g。SMB制备EPA-EE和DHA-EE具有较大的应用潜力。Eicosapentaenoic acid(EPA)and docosahexaenoic acid(DHA)are importantω-3 polyunsaturated fatty acids.Their physiological effects on humans are not exactly the same;therefore,the production of products with high-purity EPA or DHA monomers is significant.In this work,EPA ethyl ester(EPA-EE)and DHA ethyl ester(DHA-EE)were first separated using HPLC with poly(styrene-co-divinylbenzene)(PS/DVB)as the stationary phase.The effects of the mobile phase,PS/DVB particle diameter,and column temperature were systematically evaluated.The results showed that methanol is a suitable mobile phase,having a resolution of 2.75.By comparing resolutions,a PS/DVB particle diameter of 10μm was chosen;however,when the pressure drop of PS/DVB is considered,PS/DVB with a particle diameter of 20μm is more favorable for large-scale preparations.A column temperature of 40℃was found to be the most feasible for maintaining efficient separation.Second,eight semi-preparative columns(150 mm×10 mm)of PS/DVB polymer were prepared for the simulated moving bed(SMB)chromatography;the homogeneity of these columns was perfect,with a relative total column porosity error of less than 1%.Finally,an EPA-EE and DHA-EE mixture was separated using the SMB chromatography,and the contents of the extract and the raffinate were determined using GC-FID.The effects of the flow rate of ZoneⅡand ZoneⅢ,the flow rate of the feed,and the feed concentration were investigated.Under optimal conditions,EPA-EE and DHA-EE with favorable purities of 91.6%and 93.6%,respectively,were achievable.The recovery of the EPA-EE was 97.0%and the recovery of the DHA-EE was 91.6%.The productivity and solvent requirements were 5.97 g/(L\5h)and 1.52 L/g,respectively.Therefore,SMB chromatography is an attractive technology for the production of high-value products.

关 键 词：液相色谱 模拟移动床色谱 二十碳五烯酸乙酯 二十二碳六烯酸乙酯 分离 

分 类 号：O658[理学—分析化学]